Synthesis and Reactivity in Inorganic, Metal-Organic, and Nano-Metal Chemistry, 44:864–867, 2014
Copyright ꢀ Taylor & Francis Group, LLC
C
ISSN: 1553-3174 print / 1553-3182 online
DOI: 10.1080/15533174.2013.791850
Synthesis, Characterization, and Crystal Structures
of Nickel Complexes Derived from
N,Nꢀ-Bis(3,5-dichlorosalicylidene)-1,3-pentanediamine
and N,Nꢀ-Bis(3-methylsalicylidene)-1,2-ethanediamine
Gui-Hua Sheng,1 Xiao-Shan Cheng,2 Xue Wang,2 Di Huang,2 Zhong-Lu You,2
and Hai-Liang Zhu1
1School of Life Sciences, Shandong University of Technology, ZiBo, P. R. China
2Department of Chemistry and Chemical Engineering, Liaoning Normal University, Dalian 116029,
P. R. China
edge, no complexes have been reported from the Schiff base
ligand N,Nꢁ-bis(3,5-dichlorosalicylidene)-1,3-pentanediamine
(H2ClSal; Scheme 1), and two complexes have been reported
from the Schiff base ligand N,Nꢁ-bis(3-methylsalicylidene)-1,2-
ethanediamine (H2MeSal; Scheme 1).[14,15] As an extension of
our work on Schiff base complexes, we report in this article
the syntheses, characterization, and crystal structures of new
mononuclear Schiff base nickel(II) complexes, [Ni(ClSal)] (1)
and [Ni(MeSal)] (2).
Two new mononuclear Schiff base nickel(II) complexes,
[Ni(ClSal)] (1) and [Ni(MeSal)] (2) (H2ClSal = N,Nꢀ-bis(3,5-
dichlorosalicylidene)-1,3-pentanediamine; H2MeSal = N,Nꢀ-bis(3-
methylsalicylidene)-1,2-ethanediamine), have been synthesized
and characterized by elemental analyses, infrared spectra, and
single-crystal X-ray diffraction. Complex 1 crystallizes in the or-
thorhombic space group P212121, with unit cell dimensions a =
9.788(1) Å, b = 10.206(1) Å, c = 20.458(2) Å, V = 2043.7(4) Å3,
Z = 4, R1 = 0.0814, and wR2 = 0.1689. Complex 2 crystallizes in
the monoclinic space group P21/n, with unit cell dimensions a =
11.6353(5) Å, b = 11.8807(6) Å, c = 12.8241(6) Å, β = 115.213(1)◦,
V = 1603.9(1) Å3, Z = 4, R1 = 0.0243, and wR2 = 0.0675. The
Ni atoms in the complexes are four-coordinated in square planar
geometry by the N2O2 donor set of the ligands.
Keywords Crystal structure, mononuclear, nickel complex, Schiff
SCH. 1. The Schiff base ligands H2ClSal (left) and H2MeSal (right).
base
INTRODUCTION
EXPERIMENTAL
Schiff bases and their transition metal complexes have at-
tracted much attention for their importance in the fields of
coordination chemistry related to catalysis and enzymatic re-
actions, magnetism, and molecular architectures.[1–5] Nickel
is an important element in biological systems, which func-
tions as the active site of hydrolytic enzymes, such as ure-
ase.[6] Nickel complexes with Schiff bases have been proved
to possess interesting biological activities.[7–10] Recently, we
have reported some Schiff base complexes.[11–13] To our knowl-
Materials and Measurements
Commercially available 3,5-dichlorosalicylaldehyde, 3-
methylsalicylaldehyde, pentane-1,3-diamine, and ethane-1,2-
diamine were purchased from Aldrich and used without further
purification. Other solvents and reagents were made in China
and used as received. C, H, and N elemental analyses were per-
formed with a Perkin-Elmer elemental analyzer. The infrared
spectra were recorded on a Nicolet AVATAR 360 spectrometer
as KBr pellets in the 4000–400 cm−1 region.
Synthesis of the Schiff Base H2ClSal
Received 19 March 2013; accepted 27 March 2013.
3,5-Dichlorosalicylaldehyde (2.0 mmol, 0.382 g) and pentan-
1,3-diamine (1.0 mmol, 0.102 g) were dissolved in EtOH
(20 mL) with stirring. The mixture was stirred for about 30 min
at room temperature to give a large quantity of yellow precip-
itate. The product was filtered, washed with cold ethanol, and
Address correspondence to Zhong-Lu You, Department of Chem-
istry and Chemical Engineering, Liaoning Normal University, Dalian
116029, P. R. China. E-mail: youzhonglu@yahoo.com.cn and Hai-
Liang Zhu, School of Life Sciences, Shandong University of Technol-
ogy, ZiBo 255049, P. R. China. E-mail: hailiang zhu@163.com
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